CN106405715B - A kind of preparation method and applications of the PVA film for polaroid - Google Patents

A kind of preparation method and applications of the PVA film for polaroid Download PDF

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Publication number
CN106405715B
CN106405715B CN201610988577.7A CN201610988577A CN106405715B CN 106405715 B CN106405715 B CN 106405715B CN 201610988577 A CN201610988577 A CN 201610988577A CN 106405715 B CN106405715 B CN 106405715B
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polaroid
deg
preparation method
pva film
pva
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CN201610988577.7A
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Chinese (zh)
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CN106405715A (en
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陈国华
蔡福水
杨洋
黄睿
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华侨大学
厦门祥福兴胶粘制品有限公司
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    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS, OR APPARATUS
    • G02B5/00Optical elements other than lenses
    • G02B5/30Polarising elements
    • G02B5/3025Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state
    • G02B5/3033Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid
    • G02B5/3041Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid comprising multiple thin layers, e.g. multilayer stacks
    • G02B5/305Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid comprising multiple thin layers, e.g. multilayer stacks including organic materials, e.g. polymeric layers

Abstract

The invention discloses a kind of preparation methods of PVA film for polaroid, it is to be uniformly blended into water-soluble graphene quantum dots after mixing PVA powder and plasticizer, it is subsequently poured into the in the mixed solvent of methanol and distilled water composition, mixed dissolution stirs 6~12h and forms mixed solution at 70 DEG C~90 DEG C, standing and defoaming simultaneously forms a film, and obtains polarized light property after carrying out washing swelling, dyeing, extension and correction.It is that the above-mentioned PVA film with doped graphene quantum dot is made with TAC film, protective film and pressure-sensitive glue laminating the invention also discloses a kind of polaroid, the addition of graphene quantum dot can effectively prevent " indigo plant leakage " phenomenon, and improve the humidity resistance of polaroid.

Description

A kind of preparation method and applications of the PVA film for polaroid

Technical field

The present invention relates to polaroid fields, a kind of preparation method more particularly to PVA film for polaroid and its answer With.

Background technique

As information interchange and transmitting increasingly increase severely, display device has become crowd as its main carrier and material base The object of more scientist's research and probes, wherein liquid crystal display is the most widely used display device.Liquid crystal imaging must rely on Light polarizing film, the mechanism of action are as follows: the polarizing film of two panels absorption axiss in vertical state is attached to liquid crystal cell two sides, when no applied voltage When, light is unilateral without any display through polarizing.When the voltage for being applied to liquid crystal cell two sides causes the rotation of liquid crystal molecule, make to pass through The direction of vibration of the polarised light of liquid crystal layer changes, and the light of charged image part is absorbed, and shows image or number, it is seen that Polaroid is indispensable in liquid crystal imaging.

Current more common light polarizing film is iodine polarizing film, and dye series polarizing film is taken second place, and the light transmittance of light polarizing film and Degree of polarization is already close to theoretical value, but the moisture-proof of light polarizing film, hot property are wait improve.

In addition, display device often there are problems that leaking blue light.The light of blue light i.e. 400~500nm wave band, blue light can penetrate Crystalline lens reaches retina, and optical damage is caused to it, accelerates the oxidation of macular area cell, generates a large amount of free radicals, cause white A possibility that cataract or glaucoma, macular area degenerates, induces human eye macular degeneration, can increase, visual fatigue is caused to rise, developing production to physiology of eye It is raw to influence.As the problem of cognition of the people to health is more and more stronger, and blue light is leaked in display, is urgently to be resolved.

Summary of the invention

The present invention provides a kind of preparation method and applications of PVA film for polaroid, and which overcome the prior arts Polaroid present in shortcoming.

The technical solution adopted by the present invention to solve the technical problems is: a kind of preparation side of the PVA film for polaroid Method, comprising the following steps:

1) graphene quantum dot is prepared, the graphene quantum dot is water-soluble and diameter no more than 10nm;

2) it is uniformly blended into graphene quantum dot after taking PVA powder and plasticizer to mix, is subsequently poured into methanol and distilled water group At in the mixed solvent, mixed dissolution stirs 6~12h and forms mixed solution at 70 DEG C~90 DEG C, and standing and defoaming simultaneously forms a film;Its Middle PVA powder: plasticizer: methanol: the mass volume ratio of distilled water is 5~40g:0.5~10g:5~20ml:60~120ml, And concentration of the graphene quantum dot in mixed solution is 0.1ppm~10ppm;

3) by the PVA film of formation carry out washing swelling, dyeing, extension and correction after obtain polarized light property, then prior to 30~90min is dried under 30 DEG C~50 DEG C of cryogenic temperature, dries 10~60min then at 60 DEG C~80 DEG C of high-temperature temperature sections.

Preferably, concentration of the graphene quantum dot in mixed solution is 1ppm~5ppm.

Preferably, the PVA powder: plasticizer: methanol: the mass volume ratio of distilled water is 8~25g:0.5~10g:5 ~20ml:60~120ml.

Preferably, the plasticizer is glycerine, the PVA powder: glycerine: methanol: the mass volume ratio of distilled water For 5~40g:1.5~5g:5~20ml:60~120ml.

Preferably, the PVA powder: plasticizer: methanol: the mass volume ratio of distilled water is 8~25g:0.5~10g:8 ~12ml:60~120ml.

Preferably, in step 1), the preparation method of the graphene quantum dot is: the concentrated sulfuric acid and dense nitre is added in graphene In acid, it is ultrasonically treated 5~15h, the acid that distilled water is diluted and is centrifuged in removal solution is then added, obtained solid is dissolved in In the sodium hydroxide solution that pH is 10~13, moves into hydrothermal reaction kettle and react 10~14h at 180 DEG C~220 DEG C;Wherein graphite Alkene: the concentrated sulfuric acid: the mass volume ratio of concentrated nitric acid is 20~30mg:3~8ml concentrated sulfuric acid: 10~20ml concentrated nitric acid.

Preferably, in step 1), the preparation method of the graphene quantum dot is: graphene oxide is dispersed in water, Concentrated ammonia liquor mixing is added to move back into hydrothermal reaction kettle, in 280 DEG C~320 DEG C 6~10h of reaction, after being cooled to room temperature in separation Layer clear liquid;Wherein the ratio of graphene oxide and concentrated ammonia liquor is 80~120mg:20~40ml.

Preferably, in step 1), the preparation method of the graphene quantum dot is: sulfuric acid and nitric acid being mixed and are placed on ice In bath, graphene is added while stirring, sodium chlorate is slowly added to after 1~3h, adition process continues 30min~90min, to chloric acid After being completely dissolved 40~60h is stirred at room temperature in mixed solution by sodium, is centrifuged the liquid of top 2/3rds after standing overnight Obtain supernatant, adjustment supernatant pH value to 6~7 is then charged into bag filter and is placed in distilled water and is purified and removed big Size piece is concentrated and is freeze-dried.

A kind of polaroid including above-mentioned PVA film, covers the TAC film in PVA film opposing sides, covers in one of them TAC The pressure-sensing glue of the protective film of film opposite exterior lateral sides and another TAC film opposite exterior lateral sides.

Preferably, the polaroid is iodine polarizing piece or dyestuff polaroid, the PVA film with a thickness of 20~60 μm.

Compared to the prior art, the invention has the following advantages:

Graphene quantum dot of the invention has very strong quantum confined effect and edge effect, shows excellent photoelectricity Characteristic, hypotoxicity, good biocompatibility and stability etc., by the way that graphene quantum dot is added in PVA film and is made partially Mating plate can effectively improve its humidity resistance.In addition, graphene quantum dot can effectively absorb blue light, so can effectively prevent " indigo plant leakage " phenomenon, can in polaroid field development and application values.

Invention is further described in detail with reference to the accompanying drawings and embodiments;But one kind of the invention is used for polaroid The preparation method and applications of PVA film be not limited to the embodiment.

Detailed description of the invention

Fig. 1 is the flow diagram for the PVA film that PVA mixed solution preparation of the present invention has polarizing properties;

Fig. 2 is the structural schematic diagram of polaroid of the invention.

Specific embodiment

Embodiment 1

Step 1: Hummers method prepares graphene oxide.2g graphite powder is weighed respectively, pours into the 100ml concentrated sulfuric acid, gradually 10g potassium permanganate is added, is stirred at room temperature 30 minutes.35 DEG C, after constant temperature stirs 2h are adjusted the temperature to again, and 150ml distilled water is added, It is down to room temperature to solution, hydrogen peroxide is added dropwise to solution in golden yellow.Acquired solution is filtered, centrifugation be washed to it is neutral freeze again it is dry It is dry to obtain required graphite oxide.

Step 2: graphene quantum dot is prepared.By graphite oxide, high temperature reduction obtains reduction-oxidation graphite under a shielding gas Alkene.The graphene for weighing 25mg is put into round-bottomed flask, and the 5ml concentrated sulfuric acid and 15ml concentrated nitric acid is added, and is ultrasonically treated 10h.It is added 250ml distilled water is diluted, the acid being then centrifuged in removal solution.Obtained solid is dissolved in the distilled water of 40ml again and being used Sodium hydroxide solution adjusts PH to 12, then is moved into ptfe autoclave, 200 DEG C of reaction 12h.Obtained graphene quantum Point is water-soluble and diameter no more than 10nm.

Step 3: PVA film is prepared.Weigh 20g polyvinyl alcohol (PVA) powder, 3g glycerine mixes, be uniformly blended into 30mg graphene quantum dot is placed in 90ml distilled water and 10ml methanol mixed solvent, 80 DEG C of dissolutions stirring 8h, standing and defoaming, Film forming.

Step 4: PVA film moulding process.With reference to Fig. 1, by PVA film carry out washing swelling, dyeing, extension, correction so that its With polarized light property.After be respectively placed in 40 DEG C and be respectively dried with 70 DEG C of points of high and low temperature sections.Dyeing, which can be, adsorbs iodine molecule Can also will have dichromatic organic dyestuff to be adsorbed on PVA on PVA.PVA molecule is originally that any angle is random Property distribution, under certain temperature and damp condition, stress gradually deflects from force direction after stretching, and be intended to be in line shape point Cloth.As PVA molecule is arranged in a straight line along draw direction, the iodide ion or dye molecule being adsorbed on PVA layer are also with the side of having The deflection of tropism, to form long-chain.Bias is played well since iodide ion or dye molecule have, and the row of being parallel to can be absorbed The polarised light of column direction only allows the polarised light of vertical direction to pass through, to have polarized light property.

Step 5: the compacting of polaroid.According to the structure of Fig. 2, now cellulose triacetate (TAC) film 2, about 4 is pasted PVA film 3 is closed, then the outer protective film 1 of fitting PET and pressure-sensing glue 5 respectively, is finally bonded release film 6 outside in pressure-sensing glue 5.The polaroid Suitable for fields such as liquid crystal displays, wherein PVA film with a thickness of 20~60 μm.

Embodiment 2

The preparation of graphene oxide: 1. the 50ml concentrated sulfuric acid and 2g graphite, 1g sodium nitrate are added in beaker and are mixed, in magnetic force 6g potassium permanganate is slowly added under stirring, reaction is placed in 1.5h in ice-water bath.2. reaction temperature is adjusted to after the completion of low-temp reaction 35 DEG C, constant temperature is stirred to react 30min.4. 200ml deionized water after reaction, is slowly added dropwise in medium temperature, it is down to room temperature wait react, Hydrogen peroxide to solution is added, golden yellow is presented.5. the hydrochloric acid of 10% volume is added, filters, wash away6. after filtering, by filter membrane On graphite oxide distillation wash and be diluted in beaker, then be centrifuged, PH be washed till neutrality.Freeze-drying 20h must aoxidize stone Ink.7. dissolving graphite oxide by solvent of distilled water, it is poured on planetary type ball-milling 48h in ball grinder, sufficiently removing expansion carbon-coating, obtained Graphene oxide.

The preparation of graphene quantum dot: 100mg graphene oxide is dispersed in 30ml water, and 1.2ml concentrated ammonia liquor is added, will Mixed solution moves in autoclave, is warming up to 300 DEG C of reaction 8h, is cooled to room temperature, and obtained supernatant liquor is separated, i.e., Obtain the aqueous dispersions of graphene quantum dot.

The preparation of PVA film: weighing 20g polyvinyl alcohol powder, 3g glycerine mixes, and is uniformly blended into 10mg graphene Quantum dot is placed in 90ml distilled water and 10ml methanol mixed solvent, and 8h, standing and defoaming, film forming are stirred in 80 DEG C of dissolutions.

The preparation reference implementation example 1 of PVA film molding and polaroid.

Embodiment 3

Graphene oxide is prepared with traditional Hummers method: reference implementation example 1.

The preparation of graphene quantum dot: the nitric acid of the sulfuric acid of 80ml and 30ml are mixed and are added in beaker, is placed the beaker In ice bath.3g graphene is weighed, graphene is added in beaker while stirring, after two hours, weighs 30gNaClO3, It is slowly added in mixed solution (this process needs 1h), temperature is avoided to be ramping up and formed suddenly excessive ClO2Gas.When NaClO3After being completely dissolved, by mixed solution at room temperature strongly stir 48h, by reaction vessels lid loosely cover in order to Exclude the gas generated.Hereafter, which is stood overnight, the liquid of top 2/3rds is centrifuged at 5000rpm 90min., supernatant liquor pours into beaker, be drop by drop added ammonium hydroxide know PH up to 6-7. then resulting solution put into it is saturating It analyses bag (8000-14000Da), is placed in 5 days in distilled water and is purified, after 20nm thin film removing large scale piece.Finally, filtrate It is concentrated with Rotary Evaporators and is freeze-dried to obtain graphene quantum dot powder.

The preparation of PVA film: weighing 20g polyvinyl alcohol powder, 3g glycerine mixes, and is uniformly blended into 45mg graphene Quantum dot is placed in 90ml distilled water and 10ml methanol mixed solvent, and 8h, standing and defoaming, film forming are stirred in 80 DEG C of dissolutions.

The preparation reference implementation example 1 of PVA film molding and polaroid.

Above-described embodiment is only used to further illustrate a kind of preparation method of PVA film for polaroid of the invention, but It is to the above embodiments according to the technical essence of the invention any simply to repair the invention is not limited to embodiment Change, equivalent variations and modification, falls within the scope of protection of technical solution of the present invention.

Claims (10)

1. a kind of preparation method of the PVA film for polaroid, it is characterised in that the following steps are included:
1) graphene quantum dot is prepared, the graphene quantum dot is water-soluble and diameter no more than 10nm;
2) it is uniformly blended into graphene quantum dot after taking PVA powder and plasticizer to mix, is subsequently poured into methanol and distilled water composition In the mixed solvent, mixed dissolution stirs 6~12h and forms mixed solution at 70 DEG C~90 DEG C, and standing and defoaming simultaneously forms a film;Wherein PVA powder: plasticizer: methanol: the mass volume ratio of distilled water is 5~40g:0.5~10g:5~20ml:60~120ml, and Concentration of the graphene quantum dot in mixed solution is 0.1ppm~10ppm;
3) polarized light property is obtained after the PVA film of formation being carried out washing swelling, dyeing, extension and correction, then prior to 30 DEG C 30~90min is dried under~50 DEG C of cryogenic temperature, dries 10~60min then at 60 DEG C~80 DEG C of high-temperature temperature sections.
2. the preparation method of the PVA film according to claim 1 for polaroid, it is characterised in that: the graphene amount Concentration of the son point in mixed solution is 1ppm~5ppm.
3. the preparation method of the PVA film according to claim 1 for polaroid, it is characterised in that: the PVA powder: Plasticizer: methanol: the mass volume ratio of distilled water is 8~25g:0.5~10g:5~20ml:60~120ml.
4. the preparation method of the PVA film according to claim 1 for polaroid, it is characterised in that: the plasticizer is Glycerine, the PVA powder: glycerine: methanol: the mass volume ratio of distilled water is 5~40g:1.5~5g:5~20ml:60 ~120ml.
5. the preparation method of the PVA film according to claim 1 for polaroid, it is characterised in that: the PVA powder: Plasticizer: methanol: the mass volume ratio of distilled water is 8~25g:0.5~10g:8~12ml:60~120ml.
6. the preparation method of the PVA film according to claim 1 for polaroid, it is characterised in that: described in step 1) The preparation method of graphene quantum dot is: graphene being added in the concentrated sulfuric acid and concentrated nitric acid, 5~15h is ultrasonically treated, is then added The acid that distilled water is diluted and is centrifuged in removal solution, obtained solid are dissolved in the sodium hydroxide solution that pH is 10~13, It moves into hydrothermal reaction kettle and reacts 10~14h at 180 DEG C~220 DEG C;Wherein graphene: the concentrated sulfuric acid: the quality volume of concentrated nitric acid Than for 20~30mg:3~8ml concentrated sulfuric acid: 10~20ml concentrated nitric acid.
7. the preparation method of the PVA film according to claim 1 for polaroid, it is characterised in that: described in step 1) The preparation method of graphene quantum dot is: graphene oxide being dispersed in water, concentrated ammonia liquor mixing is added and moves back to hydro-thermal reaction In kettle, in 280 DEG C~320 DEG C 6~10h of reaction, supernatant liquor is separated after being cooled to room temperature;Wherein graphene oxide and concentrated ammonia liquor Ratio be 80~120mg:20~40ml.
8. the preparation method of the PVA film according to claim 1 for polaroid, it is characterised in that: described in step 1) The preparation method of graphene quantum dot is: sulfuric acid and nitric acid mixed and are placed in ice bath, is added graphene while stirring, 1~ Sodium chlorate is slowly added to after 3h, adition process continues 30min~90min, by mixed solution in room after sodium chlorate is completely dissolved Temperature is lower to stir 40~60h, is centrifuged the liquid of top 2/3rds after standing overnight to obtain supernatant, adjustment supernatant pH value is extremely 6~7, it is then charged into bag filter and is placed in distilled water and is purified and removed large scale piece, be concentrated and be freeze-dried.
9. a kind of polaroid, it is characterised in that: including PVA film as claimed in any one of claims 1 to 8, cover in PVA film phase To the TAC film on two sides, cover in the pressure-sensitive of the protective film and another TAC film opposite exterior lateral sides of one of them TAC film opposite exterior lateral sides Glue.
10. polaroid according to claim 9, it is characterised in that: the polaroid is iodine polarizing piece or dyestuff polarisation Piece, the PVA film with a thickness of 20~60 μm.
CN201610988577.7A 2016-11-10 2016-11-10 A kind of preparation method and applications of the PVA film for polaroid CN106405715B (en)

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CN107012699A (en) * 2017-03-03 2017-08-04 厦门祥福兴胶粘制品有限公司 A kind of preparation method of anti-blue light polaroid

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CN105093381A (en) * 2015-09-24 2015-11-25 深圳市华星光电技术有限公司 Quantum dot polarizer and manufacturing method thereof
WO2016025051A2 (en) * 2014-05-26 2016-02-18 William Marsh Rice University Graphene quantum dot-polymer composites and methods of making the same
CN205450329U (en) * 2016-04-01 2016-08-10 深圳市汇龙天成科技有限公司 Inclined to one side vibration -damping sheet with electrically conductive function

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101619138A (en) * 2008-06-30 2010-01-06 Lg化学株式会社 Polyvinyl alcohol film, method for preparing the same and polaroid containing the same
JP2010012778A (en) * 2008-06-30 2010-01-21 Lg Chem Ltd Method of producing polyvinyl alcohol-based film, polyvinyl alcohol-based film formed by the same, and polarizing plate provided with the same
CN102167311A (en) * 2011-03-09 2011-08-31 华侨大学 Method for preparing graphene on large scale
CN103265714A (en) * 2013-05-20 2013-08-28 西安理工大学 Polyvinyl alcohol/graphene oxide composite film preparation method
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CN205450329U (en) * 2016-04-01 2016-08-10 深圳市汇龙天成科技有限公司 Inclined to one side vibration -damping sheet with electrically conductive function

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